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利用 UHPLC-MS/MS 进行注射器清洗,检测粪肥基肥料中的硝基咪唑类和类固醇。

Syringe cleanup with UHPLC-MS/MS for nitroimidazoles and steroids detection in manure-based fertilizers.

机构信息

College of Biology and Environmental Engineering, Zhejiang Shuren University, Hangzhou, P. R. China.

A State Key Laboratory Breeding Base for Zhejiang Sustainable Plant Pest Control, Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences, Hangzhou, P. R. China.

出版信息

J Sep Sci. 2018 Aug;41(15):3089-3096. doi: 10.1002/jssc.201800322. Epub 2018 Jun 27.

DOI:10.1002/jssc.201800322
PMID:29863309
Abstract

A syringe-dispersive solid-phase extraction method was developed for the determination of seven nitroimidazoles and nine steroids in manure-based fertilizers by ultra-high performance liquid chromatography with tandem mass spectrometry. Methanol and acetonitrile were used to extract the sample, and mixed dispersive sorbents dispersed in the syringe were used for purification. The extract was separated with an HSS-T3 column and detected in positive or negative multiple reaction monitoring mode. Under the optimal conditions, the recoveries of the 16 compounds ranged from 70.3 to 112.3% at the four spiked levels (3, 10, 20, and 50 μg/kg) and the relative standard deviations ranged from 1.0 to 12.4%. The limits of detection and quantification were 0.22-0.86 and 0.73-2.87 μg/kg, respectively. This method is simple, fast, and reliable, and can be used to simultaneously screen and determine nitroimidazoles and steroids in manure-based fertilizers.

摘要

建立了一种基于针筒分散固相萃取的超高效液相色谱-串联质谱法,用于同时测定粪肥基肥料中 7 种硝基咪唑类药物和 9 种甾体类药物。甲醇和乙腈用于提取样品,针筒内混合分散的吸附剂用于净化。采用 HSS-T3 柱进行分离,在正、负离子多反应监测模式下进行检测。在最佳条件下,16 种化合物在 4 个加标水平(3、10、20 和 50μg/kg)下的回收率为 70.3%112.3%,相对标准偏差为 1.0%12.4%。检出限和定量限分别为 0.22-0.86μg/kg 和 0.73-2.87μg/kg。该方法简单、快速、可靠,可用于同时筛查和测定粪肥基肥料中的硝基咪唑类药物和甾体类药物。

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